Apparatus and process for making catalytic particles



P 1945- H. G. DALEY ETAL 2,384,455

APPARATUS AND PROCESS FOR MAKING CATALYTIC PARTICLES Filed July 15, I943INVENTORS 657W?! 6. 0415/ and Jays: 61/90/74:?0, J11

A TTORNE Y.

I Patented Sept. 11, 1945 APPARATUS AND PRO CATALYTIC Henry G. Daley,Woodbury Howard, Jr., Woodbury,

Company, Incorporated, a

Sooony-Vacuum Oil CESS FOR, MAKING PARTICLES Heights, and Jesse O. N.J., assignors to corporation of New York Application July 13, 1948,Serial No. 494,572

Claims.

This invention relates to a process and apparatus for forming adsorptivegel particles in spheroidal shape and adapted to function as a catalyst.More particularly, the invention is concerned with a novel means forsubdividing a stream of inorganic hydrosol to be formed into Theapparatus of this-invention is somewhat similar in nature to that of theprior copending application Serial, No. 477,168, flied February 25,1943, by John W. Payne, Edmund L. Sargent and Henry G. Daley. Asdescribed in that prior application, the functioning of means to supplyspheroidal gel globules.

a hydrosol to an oil bath is improved as to capacity and uniformity ofoperation by permitting the stream of hydrosol to flow onto the top of aconical divider having a plurality of grooves down its surface. Thedivider separates the stream 01 sol into a plurality of streams. eachof. which breaks up into globules of sol in the oil, the globulessetting to firm elastic gel before passing out of the oil bath into alayer of water. In the said application it is disclosed that betteroperation is obtained if the surface oi the divider is defined by asubstance, which is not wetted by water, for example, a wax. However,even the best apparatus of such type tends to accumulate gel mass on thedivider, particularly when a sol of very short gelling time-say, 5 tosecondsis used.

It has now been found that dividers of this type may be materiallyimproved by causing a water-immiscible liquid to flow down the surfaceof the divider, for example, by interposing such liquid between thedivider surface and the hydrosol. Preferably, that liquid is of suchnature that it will wet the surface of the divider, thus forming acontinuous film between the sol and the divider surface.

It is a primary object of this invention to provide means for improvingthe operation of dividers used to split a hydrosol stream. Other objectsand advantages of the invention will appear from the discussion below ofpreferred embodiments shown in the attached drawing wherein:

Figure l is a fragmentary section of apparatus for forming hydrogelspheroids according to the present invention;

Figure 2 is an enlarged view in partial section of a divider accordingto this invention;

Figure 3 is a fragmentary section oi the divider shown in Figure 2,

Figure 4 is a fragmentary section illustrating another embodiment of theinvention; and

Figure 5 is a fragmentary view of still another modification.

Referring now to Figure 1,,a mixing nozzle I0 is adapted to prepare asuitable hydrosol by intimate admixture of reactant solutions, such asacid and water glass, supplied by pipes ii and 12 from metering pumps l3and N. The hydrosol stream is discharged upon a divider ii having itslower edge at or near the suriace of a body of oil within a vessel 22.

The divider it may be of any desired form having a sloping surface witha plurality of grooves diverging downwardly from a point near the mixingnozzle it to the body of oil. Pref erably, the nozzle is conical inshape, as illustrated, since this form gives ofthe stream. Near the apexof the or other for flowing a water-immiscible liquid, for example,slots It. The cone is preferably formed cone ll,

A very satisfactory expedient is to form the cone of paraiiin wax anduse a light petroleum fraction as the water-immiscible liquid in whichthe sol sets. This petroleum fracoil, may be the same as that in whichthe globules set and thus may be circulated from the bath through a pumpi! and pipe is to emerge through orifices i8.

The details o1 the apparatus will be clear from Figures 2 and 3 whichshow the form of a conical divider in a preferred embodiment having aplurality of grooves i8 down the surface thereof. In

figures, for ease of illustration. The divider it self may be a solidbody of wax, or the like, formed on the pipe l8 which serves as a.support thereof, as well as supplying oil to the orifices it. As shownin Figure 3, the head of the pipe terminates in a cap it through whichare formed passages for oil passing to the orifices I 6.

According to an alternative embodiment shown in Figure 4, the oil orother water-immiscible fluid may be supplied to the surface oi thedivider it through a porous cap 2! communicating with and keyed to thepipe i8. In this case, all supplied under pressure by pipe l8 seepsthrough the porous cap 2! to provide 8. him of oil over the cap 2i anddown the surfaces of th divider it. In the embodiment of Figure 5, oilor other suitable liquid is supplied above the divider and flows theretofrom above. A circular supply means 25, having means 28 to supply oilthereto, is disposed in annular relation to the mixing nozzle to furnishoil to the divider surface. The manner in which this expedient operatesis not the best subdivision sloping surface, there is provided meansclearly understood. but it may be supposed that the oilpreferentiailywets the divider surface and thus forms a.nlm to which gelwill not adhere. It has been iound that gelation on the divider isgreatly reduced and occlusion of oil in the hydrogel spheres is so minoras to be unimportant.

We claim:

i. In a paratus of the class described, a conical divider, means to flowa hydrosolontc the apex thereof, a plurality of grooves diverging from apoint adiacent the apex of said cone to the lower edge thereof and meansto interpose a liquid between said divider and the hydrosol flowingthereover. comprising openings through the divider near the apex thereofand means to supply a liquid to said openings.

2. In apparatus of the class described, a conical divider, means to iiowa hydrosol onto the apex thereof. a plurality of grooves diverging froma point adjacent the apex, of said cone to the lower edge thereof andmeans to interpose a liquid between said divider and the hydrosolflowing thereover comprising a conduit coaxial with said divider cunicating with the surface thereof near the apex and means to supply aliquid to said conduit.

8. In apparatus of the class described, a conical divider, means to flowa hydrosol onto the apex thereof, a plurality of grooves diverains froma-point adjacent the apex of said cone to the lower edge thereof andmeans to interpose a liquid between said divider and the hydrosolflowing thereover comprising a porous cap on the apex of said dividerand means to supply a liquid under pressure to the interior of said cap.

4. In a processfor forming hydrogel globules by flowing a gelablehydrosol upon the apex of a conical divider; the improvement whichcomprises interposina a water-immiscible liquid which wets the surfaceof the divider between said hydrosol and said divider.

5. In a process for forming hydrogel globules by flowing a gelablehydrosol upon the apex of a conical wax divider; the improvement whichcomprises interpoeing a hydrocarbon oil between said hydrosol and saiddivider.

HENRY G. BAILEY. JBBE C. HOWARD, Jl.

